An x-ray diffractometer with controllable gas environment

Abstract

The application provides an X-ray diffraction device with controllable gas environment, which comprises an X-ray light source, a controllable sample stage and a diffraction intensity measuring device, further comprises a shell for containing the X-ray light source, the controllable sample stage and the diffraction intensity measuring device, the shell is made of a material for isolating X-rays and has air tightness; a sample transfer cabin is arranged outside the shell and provides an air-tight space for transferring samples between the outside and the controllable sample stage; a gas source is used for selectively outputting protective gas to the shell or the sample transfer cabin; a gas purification device forms a circulation loop with the shell through a first gas channel and filters the protective gas inside the shell. The X-ray diffraction device according to the application can effectively maintain the original state of the sample for a long time, accurately obtain the diffraction information of the original sample, and has compact equipment structure, simple operation and reduced cost.

Description

Technical Field

[0001] This invention relates to the field of materials testing, and in particular to an X-ray diffraction device with a controllable gas environment. Background Technology

[0002] The development of physics and materials science has always been accompanied by the continuous emergence of new materials. In the exploration of new materials and the study of their physical properties, the research on the crystal structure of materials is an indispensable first step. An X-ray diffractometer is a scientific instrument for studying the crystal structure of materials. It generally consists of core components such as an X-ray source, a sample stage, a diffraction intensity measuring device, and a goniometer. Based on the Bragg diffraction principle nλ=2dsinθ, the X-ray diffractometer utilizes the principle that the diffraction intensity of X-rays changes with the incident and exit angles of X-rays as the sample rotates, thereby enabling the testing of aspects such as the crystal structure, grain size, and crystallinity of materials. Unlike copper oxides with high-temperature superconductivity (Zeitschrift für Physik B-Condensed Matter 64,189(1986)), perovskite oxides with ferroelectric properties (Nature 358,136(1992)), and perovskite oxides with colossal magnetoresistance (Science 264,413(1994)), some novel quantum functional materials, such as topological insulators (Science 318,766(2007)), iron-based superconductors (Journal of the American Chemical Society 130,3296(2008)), zinc-arsenic-based dilute magnetic semiconductors (Nature Communications 2,422(2011)), and quantum anomalous Hall effect materials (Science 340,167(2013)), are all non-oxides. They are sensitive to air and easily react with oxygen or water vapor in the air, leading to deterioration and degradation (Reviews of Modern Physics 83, 1589 (2011); Doctoral Dissertation: Exploration and Research of Novel Quantum Functional Materials, University of Chinese Academy of Sciences (2009). Current X-ray diffractometers are typically used in air. In actual measurements, the measurement time ranges from tens of minutes to several hours to obtain a high signal-to-noise ratio. This often leads to the degradation of these new materials during sample testing due to prolonged exposure to air. Solid materials are generally classified into two main categories: bulk materials and thin film materials. Compared to bulk materials, thin film materials have a larger specific surface area, and therefore are more significantly affected and more prone to degradation.

[0003] Currently, in X-ray diffraction experiments, the method of covering the sample with a protective layer is often used to protect the sample. This includes using grease to protect various single-crystal or polycrystalline materials (Doctoral Dissertation: Exploration and Research of Novel Quantum Functional Materials, University of Chinese Academy of Sciences (2009)), and using amorphous silicon thin films to protect the thin film material under study (Nature Materials 14, 285 (2015)), thereby slowing down the deterioration of the sample during the testing process. However, these additional protective measures inevitably change the original state of the sample, making it impossible to obtain the original information of the sample, such as crystal structure information. Moreover, the complexity and cost of equipment fabrication and testing operations are relatively high. Summary of the Invention

[0004] To address the above problems, this invention provides an X-ray diffraction apparatus with a controllable gas environment, comprising: an X-ray source, a controllable sample stage, and a diffraction intensity measuring device, and further comprising:

[0005] A housing for accommodating the X-ray source, the controllable sample stage, and the diffraction intensity measuring device, the housing being made of a material for isolating X-rays and having airtightness;

[0006] A sample transfer chamber is arranged outside the housing and provides an airtight space for transferring samples between the outside and a controllable sample stage.

[0007] A gas source, the gas source being used to selectively output protective gas to the housing or the sample transfer chamber;

[0008] A gas purification device, wherein the gas purification device forms a circulation loop with the housing through a first gas channel and filters the protective gas inside the housing.

[0009] Preferably, the X-ray diffraction apparatus further includes:

[0010] A power supply for supplying power to the X-ray source;

[0011] A cooling device is used to provide heat exchange for the X-ray source;

[0012] A control device for controlling the X-ray source, the controllable sample stage, and the diffraction intensity measuring device; and wherein...

[0013] The power supply, the cooling device, and the control device are arranged on the outside of the housing.

[0014] Preferably, the housing is provided with multiple sealing joints for the power supply, the cooling device or the control device to be hermetically connected to the inside of the housing.

[0015] Preferably, the sealed connector for connecting the power source also provides electrical isolation between the power source and the housing.

[0016] Preferably, the sample transfer chamber has a first valve communicating with the outside and a second valve communicating with the inside of the housing.

[0017] Preferably, the controllable sample stage and the diffraction intensity measuring device are each able to rotate along the same rotation axis, and their respective angular velocities are controllable.

[0018] Preferably, the housing has a cuboid structure, and the sidewall of the housing has an airtight glove interface.

[0019] Preferably, a movable plate is also arranged on the outer side of the housing, wherein the movable plate can cover or expose the glove interface, and the movable plate is made of a material for isolating X-rays.

[0020] Preferably, the housing includes an observation window made of a transparent material for isolating X-rays.

[0021] Preferably, the gas purification device includes:

[0022] A purification column module is used to purify the protective gas;

[0023] A blower module is used to blow air in the first gas channel to form the circulation loop;

[0024] The sensor module is coupled to the first gas channel and is used to obtain the oxygen content, water vapor content and pressure value respectively;

[0025] The controller module is used to receive the oxygen content, water vapor content and pressure values ​​output by the sensor module, and to control the on / off state of the fan module.

[0026] Preferably, the gas purification device further includes:

[0027] A vacuum pump is used to evacuate the sample transfer chamber;

[0028] A second gas channel connects the sample transfer chamber, the vacuum pump, and the gas source; and

[0029] At least one gas valve is distributed in the second gas channel, which is used to control the communication status between the sample transfer chamber, the vacuum pump, the first gas channel and the gas source;

[0030] The controller module is also used to control the on / off state of the vacuum pump and the at least one gas valve.

[0031] Preferably, the first operating mode of the controller module controls the at least one gas valve so that only the sample transfer chamber is connected to the vacuum pump, and controls the vacuum pump to evacuate the sample transfer chamber;

[0032] The second operating mode of the controller module controls the at least one gas valve so that only the sample transfer chamber is connected to the gas source to fill the sample transfer chamber with the protective gas;

[0033] The third operating mode of the controller module controls the at least one gas valve such that only the housing, the first gas passage, and the gas source are connected to fill the interior of the housing with the protective gas.

[0034] The X-ray diffraction apparatus of the present invention constructs a miniaturized sealed space based on existing X-ray diffraction apparatuses to maintain a high-purity protective gas environment for extended periods. Therefore, it provides a novel X-ray diffraction measurement method for various air-sensitive sample materials. This method can effectively prevent the degradation of the sample while obtaining higher precision diffraction data and experimental accuracy during long-term X-ray diffraction experiments, without altering the sample's original state. This allows for accurate acquisition of information such as the sample's original crystal structure, grain size, and crystallinity. Furthermore, existing X-ray diffractometers are bulky, making it impractical to place them entirely in a non-air environment; and their outer shielding lead plate lacks airtightness, making it difficult to control the gas environment surrounding the aforementioned air-sensitive materials during X-ray diffraction experiments. The X-ray diffraction apparatus designed in various preferred embodiments of the present invention compresses the main structure into a smaller, airtight chamber, providing higher testing accuracy while making the structure more compact, increasing space utilization, and reducing experimental costs. Attached Figure Description

[0035] The embodiments of the present invention will be further described below with reference to the accompanying drawings, wherein:

[0036] Figure 1 A schematic diagram of the structure of an X-ray diffraction apparatus according to a preferred embodiment of the present invention is shown;

[0037] Figure 2 A schematic diagram showing the connection relationships of the various components in the gas handling unit of an X-ray diffraction apparatus is provided.

[0038] Figure 3 As shown Figure 1 The diagram shows the internal structure of the housing and auxiliary devices in the X-ray diffraction apparatus. Detailed Implementation

[0039] Figure 1A schematic diagram of an X-ray diffraction apparatus with a controllable gas environment according to a preferred embodiment of the present invention is shown. The X-ray diffraction apparatus 1 mainly includes an X-ray source 101, a controllable sample stage 102, and a diffraction intensity measuring device 103. It also includes a housing 10, a transfer chamber 20, a gas handling device 30, and auxiliary devices 40. The housing 10 is used to house the X-ray source 101, the controllable sample stage 102, and the diffraction intensity measuring device 103.

[0040] like Figure 1 As shown, the housing 10 is rectangular in shape and is a sealed cavity, constructed by welding six lead-containing metal plates together, with the joints sealed with adhesive for further sealing. The lead-containing metal plates are approximately 15mm thick to ensure X-ray blocking. Figure 1 The first sidewall 11, the second sidewall 12, and the third sidewall 13 opposite to the second sidewall 12 can be observed. Furthermore, the connecting wall 14 between the housing 10 and the auxiliary device 40... Figure 1 The details are obscured and will be described below. Glove interfaces 111 and 112 are arranged laterally at intervals on the first sidewall 11 (here, the direction perpendicular to the second sidewall 12 and the third sidewall 13 and parallel to the first sidewall 11 is defined as lateral), and the glove interfaces 111 and 112 are sealed to the operating gloves. Figure 1 (Not shown), the operating glove extends into the housing 10 and airtightly isolates the interior of the housing 10 from the exterior. Movable plates 114 and 115 are also arranged on the first sidewall 11. Movable plates 114 and 115 have the same structure; here, only movable plate 114 is described as an example: Movable plate 114 can slide laterally or open by hinge rotation. When it moves to a first position near the edge of the first sidewall 11, the outer side of the glove interface 111 is completely unobstructed; when it moves to a second position near the center of the first sidewall 11, the outer side of the glove interface 111 is completely obstructed. Figure 1 The dotted circle in the diagram illustrates the glove interface 111, which is obscured by the movable plate 114. The cavity walls of the housing 10, the movable plates 114 and 115, can be made of various materials capable of isolating X-rays; in this embodiment, they are made of thick lead plates. An observation window 116 is provided on the first sidewall 11. The orientation of the observation window 116 allows for convenient observation of the components of the housing 10 and the operation of the glove. The observation window 116 is made of leaded glass or other materials capable of isolating radiation waves while allowing visible light to pass through. It measures approximately 500 mm in length, 300 mm in width, and 15 mm in thickness. The leaded glass is sealed to the surrounding leaded metal plate using a rubber ring. A similar movable plate can also be configured on the outside of the observation window 116 to further isolate X-rays when observation is not required.

[0041] like Figure 1As shown, the transfer chamber 20 is connected to and fixed to the second side wall 12 of the housing 10. The transfer chamber 20 is a cavity structure, with one end connected to the interior of the housing 10 and having a valve 201, and the other end also having a valve 202 to allow samples to be introduced from the outside and then sealed. Therefore, samples can be transferred to the interior of the housing 10 through the transfer chamber 20. The transfer chamber 20 is connected to the pipe 51 through the pipe 53 and the gas valve 531 on the pipe 53, and to the gas processing device 30 through the pipe 54 and the gas valve 541 on the pipe 54.

[0042] like Figure 1 As shown, the gas processing device 30 mainly includes a purification column module 31, a fan module 32, a vacuum pump module 33, a control module 34, a first sensor 361, a second sensor 362, a third sensor 363, and a protective gas source 37. The housing 10, pipe 52, purification column module 31, fan module 32, and pipe 51 are connected end-to-end to form a gas flow circulation loop. Preferably, pipes 51 and 52 are arranged relatively close to the body diagonal of the housing 10 at their connection points. The protective gas source 37 can be a gas storage cylinder or an external gas supply facility, which is connected to pipe 55. The gas processing device 30 is used to draw gas from inside the housing 10 through the second pipe 52, process it to generate (including filtering or replacement) a single-component gas, and then discharge it back into the housing 10 through pipe 51. This cyclical process completes the control of the gas composition inside the housing 10. The gas processing device 30 also includes multiple sensors for outputting detection signals, including a first sensor 361, which is arranged on pipe 51 and used to obtain the gas pressure signal inside pipe 51; a second sensor 362, which is arranged on pipe 52 and used to obtain the oxygen content signal inside pipe 52; and a third sensor 363, which is arranged on pipe 52 and used to obtain the water vapor content signal inside pipe 52. The suction end of the vacuum pump module 33 is connected to pipe 54 and thereby to the transfer chamber 20, and is used to evacuate the interior of the transfer chamber 20. Pipes 51 and 52, which are used to realize the protective gas circulation loop, are collectively referred to as the first gas pipes; while the remaining auxiliary pipes are collectively referred to as the second gas pipes.

[0043] like Figure 1 As shown, the auxiliary device 40 is equipped with multiple devices for assisting the operation of the X-ray source 101, the controllable sample stage 102, and the diffraction intensity measuring device 103 inside the housing 10, including a transformer 41, a cooling device 42, and a control device 43. Its structural features will be described later. Figure 3 As introduced in the text.

[0044] Figure 2A schematic diagram showing the connection relationship of the various components in the gas processing device 30 is shown. The gas processing device 30 also includes a pipe 53 with a gas valve 531, a pipe 54 with a gas valve 541, a pipe 55 with gas valves 553 and 554, and a branch pipe 552. The protective gas in the gas source 37 can be one of the inert gases; in this embodiment, nitrogen is used. The purification column module 31 has a first interface 311, a second interface 312, a third interface 313, and a fourth interface 314 that can be opened or closed. The first interface 311 of the purification column module 31 is connected to the pipe 52 for drawing in gas from inside the housing 10; the second interface 312 is connected to the suction end of the fan module 32; the third interface 313 and the fourth interface 314 are used to connect to an external reducing gas source (…). Figure 2 (Not shown in the image); the interior of the purification column module 31 is filled with materials such as copper catalyst and molecular sieve for adsorbing oxygen and water vapor. The exhaust end of the fan module 32 is connected to the interior of the housing 10 via a pipe 51, for discharging the gas drawn in from its intake end to the housing 10. The inlet pipe 55, which connects to the external protective gas source 37, is connected to pipe 54 and is located between the gas valve 541 and the vacuum pump module 33; the branch pipe 552 connects the inlet pipe 55 and pipe 51, wherein the interface between the branch pipe 552 and pipe 51 is located between the interface between pipe 53 and pipe 51 and the fan module 32. The inlet pipe 55 has a gas valve 553 and a gas valve 554, with the gas valve 554 arranged in the portion of the inlet pipe 55 between the protective gas source 37 and the branch pipe 552, and the gas valve 553 arranged in the portion of the inlet pipe 55 between the branch pipe 552 and pipe 54.

[0045] The input terminals of the control module 34 are connected to the first sensor 361, the second sensor 362, and the third sensor 363 via circuitry, and the output terminals of the control module 34 are connected to the fan module 32, the vacuum pump module 33, and the air valves 531, 541, 553, and 554. Operators can use the control module 34 to read the air pressure signal output by the first sensor 361, the oxygen content signal output by the second sensor 362, and the water vapor content signal output by the third sensor 363, and control the operating status of the fan module 32, the vacuum pump module 33, and the air valves 531, 541, 553, and 554.

[0046] Figure 3 As shown Figure 1This diagram illustrates the connection between the housing 10 and the auxiliary device 40 in the X-ray diffraction apparatus. Only the internal components of the housing 10 and auxiliary device 40, and the connecting wall 14 between them, are shown, while the remaining outer walls are removed. The housing 10 houses an X-ray source 101, a controllable sample stage 102, and a diffraction intensity measuring device 103. The controllable sample stage 102 can be controlled to rotate along a first normal direction at a first angular velocity and has a precise angle measurement function. The diffraction intensity measuring device 103 can rotate along the first normal direction at a second angular velocity. The first normal direction, the first angular velocity, and the second angular velocity can be adjusted; preferably, the second angular velocity is twice the first angular velocity. The connecting wall 14 is equipped with a first circuit sealing joint 141, a second circuit sealing joint 142, and a pipe sealing joint 143.

[0047] like Figure 3 As shown, the transformer 41 is connected to the X-ray source 101 via a first circuit-sealed connector 141 and high-voltage cables 411 at both ends. It obtains power from an external power source and performs a voltage boosting operation before supplying it to the X-ray source 101. The first circuit-sealed connector 141 provides electrical insulation at a higher voltage between the connecting wall 14 and the high-voltage cables 411, while simultaneously sealing the high-voltage cables 411 to the connecting wall 14. The cooling device 42 has circulation pipes 421 and 422, both of which extend hermetically into the housing 10 via a pipe-sealed connector 143. The other ends of the circulation pipes 421 and 422 are connected and contact the heat dissipation surface of the X-ray source 101. Therefore, the cooling device 42 provides heat exchange with the X-ray source 101 by circulating coolant between the circulation pipes 421 and 422. The multiple output terminals of the control device 43 are respectively connected to the X-ray source 101, the controllable sample stage 102, and the diffraction intensity measuring device 103 via independent circuit cables 431, 432, and 433 and hermetically sealed via the second circuit sealing connector 141, so as to control them respectively. The first or second circuit sealing connector may be made of epoxy resin material wrapped around metal wire terminals.

[0048] The following is combined Figure 1 The working process of the X-ray diffraction device of the present invention is described.

[0049] (1) Formation process of protective gas environment inside the shell: The mixed gas environment (atmospheric environment) inside the shell 10 is replaced with a single gas environment containing only one protective gas. First, the gas environment control device 1 is powered on and started, and the first interface 311, the second interface 312, the third interface 313 and the fourth interface 314 of the purification column module 31 are closed. The fan module 32 is turned off through the control module 34, the gas valves 553 and 541 are closed, the gas valve 531 is closed and the gas valve 554 is opened. As a result, the external protective gas source 37 is connected to the shell 10. Since the external protective gas source 37 stores a single protective gas with a pressure greater than atmospheric pressure, a unidirectional airflow is formed and quickly fills the shell 10. After a period of time, the original air inside the shell 10 is basically discharged and only the single protective gas is filled. At this time, the circulation operation begins. First, the first interface 311 and the second interface 312 of the purification column module 31 are opened, and the fan module 32 is turned on, thus forming a circulating airflow. This airflow travels along the housing 10, through the pipe 52, the purification column module 31, and the fan module 32, and returns to the housing 10 along the pipe 51. Therefore, the protective gas, which may contain oxygen or water vapor within the housing 10, is absorbed or filtered when it flows through the copper catalyst, molecular sieve, and other substances inside the purification column module 31. Thus, only high-purity protective gas is discharged from the second interface 312 of the purification column module 31. During the circulation process, the first sensor 361, the second sensor 362, and the third sensor 363 output the air pressure value in the pipe 51, the oxygen content value inside the pipe 52, and the water vapor content value to the control module 34 in real time, respectively. The operator can read these three parameters. This process ends when the oxygen content signal output by the second sensor 362 and the water vapor content signal output by the third sensor 363, as read by the operator through the control module 34, are both less than 0.1 ppm.

[0050] (2) Sample introduction process: First, the sample to be tested, such as a newly prepared polycrystalline sample, single crystal sample, or thin film sample that has not been exposed to air, is introduced into the transfer chamber 20 from an external protective gas environment. Specifically, valve 201 at the connection between the transfer chamber 20 and the shell 10 is closed, valve 202 on the opposite side is opened, and the sample is placed inside from the outside. Then, valve 202 is closed. Next, the control module 34 controls the closing of gas valve 531, the closing of gas valve 553, and the starting of vacuum pump module 33, opening gas valve 541, so that vacuum pump module 33 evacuates the transfer chamber 20. Then, the control module 34 keeps gas valve 553 closed and opens gas valves 554 and 531, and manually closes the second interface 312 of purification column module 31 to fill the transfer chamber 20 with protective gas. Repeating the above steps 3 to 5 times can ensure that the purity of the protective gas in the transfer chamber 20 is high. Finally, valve 201 is opened, and the operator transfers the sample to the controllable sample stage 102 through the operating gloves at glove interfaces 111 and 112, and then closes valve 201. After the operation is completed, movable plates 114 and 115 are moved to their respective second positions to completely cover the outside of glove interfaces 111 and 112.

[0051] (3) X-ray diffraction experiment process: By operating and controlling the control device 43 in the auxiliary device 40 on the atmospheric side, the X-ray source 101 and the diffraction intensity measuring device 103 test the sample on the controllable sample stage 102 within the shell 10 filled with a single protective gas environment. The X-ray source is controlled to irradiate the sample on the sample stage 102, and then the sample is rotated relative to the X-ray source along a specific spatial angle direction with the sample stage having an angle measuring function. At the same time, the diffraction intensity measuring device is controlled to rotate along the same spatial angle direction at twice the speed of the goniometer, according to the diffraction relationship required by Bragg's law, and diffraction data are collected along the entire diffraction direction. The relationship between the intensity and the rotation angle recorded by the diffraction intensity measuring device is thus obtained as the X-ray diffraction pattern of the sample, thereby obtaining useful information such as the sample's precise crystal structure, lattice spacing, deformation, stress, and crystal orientation. During the X-ray diffraction experiment, although the shell 10 is a sealed cavity, there are still tiny gaps in its sidewalls, so molecular diffusion occurs. Since X-ray diffraction typically takes tens of minutes to several hours, impurities in the external atmosphere that can easily affect the sample, such as oxygen or water vapor, will gradually diffuse into the interior of the housing 10. The gas handling device performs a circulating filtration operation in this situation.

[0052] (4) Sample transfer process: After the test is completed, firstly, valve 201 is opened, and the operator uses the operating gloves through glove interfaces 111 and 112 to transfer the sample from the controllable sample stage 102 to the transfer chamber 20, and then closes valve 201. Then, valve 202 is opened, the sample is taken out, and transferred to other external protective gas environments.

[0053] In addition to the above-described operation of the X-ray diffraction apparatus of the present invention, if the adsorbent materials such as copper catalyst and molecular sieve filled in the purification column module 31 have become saturated and cannot effectively purify the protective gas, the first interface 311 and the second interface 312 of the purification column module 31 can be closed; the third interface 313 and the fourth interface 314 can be connected to an external reducing gas source to form a circulating gas channel. When the reducing gas in the reducing gas source enters the purification column module 31 and comes into contact with the adsorbent materials such as copper catalyst and molecular sieve, a reduction reaction occurs, thereby restoring the adsorption capacity of the adsorbent materials such as copper catalyst and molecular sieve.

[0054] In other embodiments of the invention, the transfer chamber 20 can be designed as a detachable structure at both ends, so that the sample can be placed in the transfer chamber 20 filled with protective gas in another external protective gas environment first, and then the sealed transfer chamber 20 can be connected to the housing 10 to transfer the sample into the housing 10. This more effectively prevents potential contamination by impurity gases during the sample transfer into the housing 10.

[0055] In the X-ray diffraction apparatus described in other embodiments of the present invention, the connections between the various top plates, bottom plates, or side plates of the housing 10 can be further sealed with adhesive to increase its airtightness. Rubber rings can also be used to seal the various interfaces, joints, or between the leaded glass and leaded metal plate of the observation window. Furthermore, the cavity of the housing 10 can be designed as a spherical shell, making it easier to manufacture in one piece to increase pressure resistance and sealing performance. The air valve can be an electric valve controlled by the control module 34, or it can be replaced with a manual valve to ensure reliability and economy.

[0056] In the X-ray diffraction apparatus described in other embodiments of the present invention, each gas valve and the two valves of the transfer chamber 20 are controlled by the control module 34. Therefore, the control module 34 can control the gas environment control device 1 to enter working state 1 or working state 2, or close each valve and stop the fan circulation, based on the values ​​received from the first sensor 361, the second sensor 362 and the third sensor 363 and multiple upper or lower threshold values ​​pre-stored in the circuit. For example, when the oxygen content signal output by the second sensor 362 is greater than the preset first oxygen content upper limit threshold, or when the water vapor content signal output by the third sensor 363 is greater than the preset first water vapor content upper limit threshold, the control module 34 determines and controls the gas environment control device 1 to enter working state 2 to perform a cyclic filtration operation; when the oxygen content signal output by the second sensor 362 is greater than the preset second oxygen content upper limit threshold (the second oxygen content upper limit threshold is greater than the first oxygen content upper limit threshold), or when the water vapor content signal output by the third sensor 363 is greater than the preset second water vapor content upper limit threshold (the second water vapor content upper limit threshold is greater than the first water vapor content upper limit threshold), the control module 34 determines and controls the gas environment control device 1 to enter working state 1 to perform a gas washing operation to more thoroughly replace the mixed gas environment with a single gas environment. If the oxygen content signal output by the second sensor 362 is still greater than the second oxygen content upper limit threshold after a predetermined time period, or the water vapor content signal output by the third sensor 363 is still greater than the second water vapor content upper limit threshold after a predetermined time period, the control module 34 will determine and close all air valves and control the fan to stop, and issue an audible and visual warning signal to the outside world.

[0057] While the present invention has been described through preferred embodiments, it is not limited to the embodiments described herein, and various changes and modifications are made without departing from the scope of the invention.

Claims

1. An X-ray diffraction device with a controllable gas environment, comprising: The X-ray source, the controllable sample stage, and the diffraction intensity measuring device are characterized by further comprising: A housing for accommodating the X-ray source, the controllable sample stage, and the diffraction intensity measuring device, the housing being made of a material for isolating X-rays and having airtightness; A sample transfer chamber is arranged outside the housing and provides an airtight space for transferring samples between the outside and a controllable sample stage. The sample transfer chamber is designed to be detachable at both ends. A gas source stores a single protective gas with a pressure greater than atmospheric pressure. The gas source is used to selectively output the protective gas to the shell or the sample transfer chamber. When the gas source outputs the protective gas to the shell, the protective gas forms a unidirectional airflow to expel the original air inside the shell, so that the shell is filled only with the protective gas. A gas purification device, wherein the gas purification device forms a circulation loop with the housing through a first gas channel and filters the protective gas inside the housing; A power supply for supplying power to the X-ray source; Cooling device for providing heat exchange to the X-ray source; and A control device is used to control the X-ray source, the controllable sample stage, and the diffraction intensity measuring device. The power supply, the cooling device, and the control device are arranged on the outside of the housing. The housing is provided with multiple sealing joints for the power supply, the cooling device, or the control device to be airtightly connected to the inside of the housing. The gas purification device includes: A vacuum pump is used to evacuate the sample transfer chamber; The second gas channel connects the sample transfer chamber, the vacuum pump, and the gas source. The second gas channel includes a branch channel connected to the first gas channel. The gas source outputs the protective gas to the housing sequentially through a portion of the second gas channel, the branch channel, and a portion of the first gas channel. A sensor module, coupled to the first gas channel, is used to obtain oxygen content, water vapor content, and pressure values, respectively; and The controller module is used to receive the oxygen content, water vapor content, and pressure value output by the sensor module. When the oxygen content is greater than a preset first upper limit threshold or when the water vapor content is greater than a preset first upper limit threshold, the controller module causes the gas purification device to filter the protective gas inside the housing. When the oxygen content is greater than a preset second upper limit threshold or when the water vapor content is greater than a preset second upper limit threshold, the controller module causes the gas source to output the protective gas to the housing, wherein the second upper limit threshold is greater than the first upper limit threshold and the second upper limit threshold is greater than the first upper limit threshold.

2. The X-ray diffraction apparatus according to claim 1, characterized in that, The sealed connector that provides the power supply connection also provides electrical isolation between the power supply and the housing.

3. The X-ray diffraction apparatus according to claim 1, characterized in that, The sample transfer chamber has a first valve that communicates with the outside and a second valve that communicates with the inside of the housing.

4. The X-ray diffraction apparatus according to claim 1, characterized in that, The controllable sample stage and the diffraction intensity measuring device can each rotate along the same rotation axis, and their respective angular velocities can be controlled.

5. The X-ray diffraction apparatus according to claim 1, characterized in that, The housing has a cuboid structure, and the side wall of the housing has an airtight glove interface.

6. The X-ray diffraction apparatus according to claim 5, characterized in that, The outer side of the housing is also provided with a movable plate, wherein the movable plate can cover or expose the glove interface, and the movable plate is made of a material for isolating X-rays.

7. The X-ray diffraction apparatus according to claim 1, characterized in that, The housing includes an observation window made of a transparent material for isolating X-rays.

8. The X-ray diffraction apparatus according to claim 1, characterized in that, The gas purification device includes: A purification column module is used to purify the protective gas; A blower module is used to blow air into the first gas channel to form the circulation loop. The controller module is used to control the on / off state of the fan module.

9. The X-ray diffraction apparatus according to claim 8, characterized in that, The gas purification device also includes: At least one gas valve is distributed in the second gas channel, which is used to control the communication status between the sample transfer chamber, the vacuum pump, the first gas channel and the gas source; The controller module is also used to control the on / off state of the vacuum pump and the at least one gas valve.

10. The X-ray diffraction apparatus according to claim 9, characterized in that, The first operating mode of the controller module controls the at least one gas valve so that only the sample transfer chamber is connected to the vacuum pump, and controls the vacuum pump to evacuate the sample transfer chamber. The second operating mode of the controller module controls the at least one gas valve so that only the sample transfer chamber is connected to the gas source to fill the sample transfer chamber with the protective gas; The third operating mode of the controller module controls the at least one gas valve such that only the housing, the first gas passage, and the gas source are connected to fill the interior of the housing with the protective gas.

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